色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 32-39.DOI: 10.3724/SP.J.1123.2018.07019

• 特别策划：南京海关动植物与食品检测中心专栏 • 上一篇    下一篇

气相色谱-负化学源-质谱法检测水中10种全氟羧酸化合物

王晓研1, 沈伟健2, 王红2, 余可垚2, 吴斌2, 胡国绅2, 杨功俊1   

  1. 1. 中国药科大学药学院, 江苏 南京 210009;
    2. 南京海关动植物与食品检测中心, 江苏 南京 210009
  • 收稿日期:2018-07-20 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 杨功俊E-mail:yanggongjun888@163.com.
  • 基金资助:

    长三角课题（17395810102）；中国-马来西亚合作课题（PORTSIM061/2017）.

Determination of 10 perfluorinated carboxylic acid compounds in water by gas chromatography-mass spectrometry coupled with negative chemical ionization

WANG Xiaoyan1, SHEN Weijian2, WANG Hong2, YU Keyao2, WU Bin2, HU Guoshen2, YANG Gongjun1   

  1. 1. College of Pharmacy, Chian Pharmaceutical University, Nanjing 210009, China;
    2. Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210009, China
  • Received:2018-07-20 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    Yangtze River Delta Project (No. 17395810102); China-Malaysia Cooperation Project (No. PORTSIM061/2017).

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摘要：

建立了气相色谱-负化学源-质谱（GC-NCI-MS）检测水中10种全氟羧酸化合物的分析方法。使用硅烷衍生化试剂N-甲基-N-三甲基硅基三氟乙酰胺（MSTFA）对全氟羧酸化合物进行衍生化，水样经弱阴离子交换固相萃取柱净化富集后进样。实验优化了样品前处理、衍生化和仪器条件。结果表明，10种全氟羧酸化合物在0.1~10 mg/L范围内线性关系良好，相关系数为0.9956~0.9993；方法的检测限（LOD）和定量限（LOQ）分别为0.5~1.5 μg/L和1.5~4.5 μg/L。在空白水样中进行了3个添加水平的加标回收试验，10种全氟羧酸化合物的平均回收率为70.2%~112.6%，相对标准偏差（RSD）为2.1%~14.5%（n=6）。该法原理简单，灵敏度高，准确、精密，可实现水体中10种全氟羧酸化合物同时检测的要求。

关键词: 负化学源, 固相萃取, 气相色谱-质谱, 全氟羧酸化合物, 水

Abstract:

A method was developed for the simultaneous determination of 10 perfluorinated carboxylic acid compounds in water by gas chromatography-mass spectrometry coupled with negative chemical ionization (GC-NCI-MS). Perfluorinated carboxylic acid compounds were derivatized by trifluoro-N-methyl-N-(trimethylsilyl) acetamide (MSTFA) as the trimethylsilyl derivatization reagent. The water sample was purified and enriched through a weak anion exchange solid phase extraction column and analyzed via GC-NCI-MS. The sample pretreatment, derivation and instrument conditions were optimized. The results showed that the linearity of the 10 perfluorinated carboxylic acid compounds was good in the range of 0.1-10 mg/L with correlation coefficients of 0.9956-0.9993. The limits of detection (LODs) and limits of quantification (LOQs) were 0.5-1.5 μg/L and 1.5-4.5 μg/L, respectively. The spiked recoveries of the blank samples ranged from 70.2% to 112.6% with the relative standard deviations (RSDs) between 2.1% and 14.5% (n=6). The method is simple, sensitive, accurate and precise, and can be used to detect the 10 perfluorinated carboxylic acid compounds in water.

Key words: gas chromatography-mass spectrometry (GC-MS), negative chemical ionization (NCI), perfluorinated carboxylic acid compounds, solid phase extraction (SPE), water

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